Thermal analysis automated systems

An Automated Thermal Analysis System for Reaction Kinetics," A.F. Kah, M.E. Koehler, T.H. Grentzer, T.F. Niemann, and T. Provder, Computer Applications... 

Kah, A. F. Koehler, M. E. Grentzer, T. H. Niemann, T. F. Provder, T. "An Automated Thermal Analysis System for Reaction Kinetics" in "Computer Applications in Applied Polymer Science" Provder, T., Ed. ACS SYMPOSIUM SERIES No. 197, American Chemical Society Washington, D.C., 1982 pp. 197-311. 

An Automated Thermal Analysis System for Reaction Kinetics... 

A DuPont Model 990 Thermal Analysis Console with Model 910 DSC accessory was interfaced to a minicomputer system by means of a microcomputer for automated data collection. A program to provide the analysis of reaction kinetics data by the single dynamic scan method for DSC kinetics was developed. Features of this program include a fit of the data to a single equation by multiple regression techniques to yield the reaction order, the energy of activation and the Arrhenius frequency factor. The rate constant k(T) is then calculated and conversion data as a function of time and temperature can be generated at the operator s option. 

X-ray powder diffraction patterns were obtained by using a Philips PW 1729 diffraction automated with an ADP system. Cu Ka operated at 40 Kv and 30 ma was the x-ray source. Samples were scanned from 20 = 3 to 70 Thermal gravimetric analysis (TGA) was done by using a Du Pont 9900 thermal analysis system. IR spectroscopy was performed on a Bomem DA 3.02 FT-IR spectrometer. B, Al, and Mg were determined by ICP spectroscopy with the solutions obtained by dissolving the sample in 6N HCl. 

Yuen HK, Mappes GW, Grote WA. An automated system for simultaneous thermal analysis and mass spectrometry. Thermochim Acta. 1982 52 143-53. 

Most thermal analysis studies today are conducted with commercial instruments. Manufactures have striven to provide complete systems capable of a wide range of analyses and frequently sharing modular components. Naturally, this is a market-driven phenomenon, and the current driving forces are speed, miniaturization, and automation. The goals of a modern industrial quality control facility, a state-of-the-art research institution, or those of a teaching laboratory are quite different. This difference leads to a broad spectrum of available instrumentation in terms of ultimate capabiUties, simplicity, and cost. 

Another step in laboratory automation to be achieved is the conversion of standard chemical procedures such as titrations or thermal gravimetric analysis, into unit laboratory operations. A procedure could then be selected from these laboratory operations by an expert system and translated by the system to produce a set of iastmctions for a robot. The robot should be able to obey specific iastmctions, such as taking a specified sample aliquot and titrating it using a specified reagent. 

Headspace analysis involves examination of the vapours derived from a sample by warming in a pressurized partially filled and sealed container. After equilibration under controlled conditions, the proportions of volatile sample components in the vapours of the headspace are representative of those in the bulk sample. The system, which is usually automated to ensure satisfactory reproducibility, consists of a thermostatically heated compartment in which batches of samples can be equilibrated, and a means of introducing small volumes of the headspace vapours under positive pressure into the carrier-gas stream for injection into the chromatograph (Figure 4.25). The technique is particularly useful for samples that are mixtures of volatile and non-volatile components such as residual monomers in polymers, flavours and perfumes, and solvents or alcohol in blood samples. Sensitivity can be improved by combining headspace analysis with thermal desorption whereby the sample vapours are first passed through an adsorption tube to pre-concentrate them prior to analysis. 

Borusiewicz, R., Zadora, G., Zigba-Palus, J. Application of head-space analysis with passive adsorption for forensic purposes in the automated thermal desorption-gas chromatography-mass spectrometry system. Chromatographia 60, 133-142 (2004)... 

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